HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 178434238, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 178434239 | HCID 178434239 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178434238 | HCID 178434238 | — |
Reaction Steps
A solution of 100 mg (0.277 mmol) 2,6-bis(difluoromethyl)-4-(3-methyl-1H-indazol-5-yl)-1,4-dihydropyridine-3,5-dicarbonitrile (Example 13) in DMF (1.5 ml) was cooled to 0° C., and 108 mg (0.33 mmol) caesium carbonate were added at this temperature. After stirring for 30 min, 21 μl (0.33 mmol) methyl iodide were added dropwise at room temperature, and the mixture was stirred at rt overnight. After this, additional methyl iodide (20 μl) was added, and stirring at rt was continued for further 48 h. The reaction mixture was then filtered, and the filtrate was directly purified by preparative RP-HPLC (acetonitrile/water+0.1% TFA isocratic 40:60 v/v) to give 12 mg (11% of th.) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422263B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-8a48310868ac4cb68e482b69f1058e72 |
| Source note | uspto-grants-2016_08 |